Tetrahydrofuran → (2-Chloropyridin-4-yl)methanol
反応式
O1CCCC1.[Cl:6][C:7]1[CH:8]=[C:9]([CH:13]=[CH:14][N:15]=1)[C:10](O)=[O:11]>C(OCC)(=O)C>[Cl:6][C:7]1[CH:8]=[C:9]([CH2:10][OH:11])[CH:13]=[CH:14][N:15]=1参加物
4
実験手順
Borane-dimethyl sulfide complex (14.30 mL, 14.30 mmols) was added to tetrahydrofuran solution of 2-chloroisonicotinic acid (17.56 g, 11.5 mmols) under cooling with ice, and stirred at room temperature for 2.5 days, followed by further an hour's stirring at 50° C. Cooling the reaction liquid to room temperature, ethyl acetate was added, followed by washing with saturated aqueous ammonium chloride solution and saturated brine and drying over anhydrous sodium sulfate. Concentrating the solvent under reduced pressure, the tide compound (15.0 g, 93%) was obtained.
後処理
- temperatureunder cooling with ice
- waitfollowed by further an hour
- stirring's stirring at 50° C
- temperatureCooling
- customthe reaction liquid to room temperature
- washby washing with saturated aqueous ammonium chloride solution and saturated brine
- dry with materialdrying over anhydrous sodium sulfate
- concentrationConcentrating the solvent under reduced pressure
出典と根拠
- ORDレコード
- ord-3fa492606d864acd8a6b58ac8a2f15f7
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07732456B2
反応ノート
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